超高效液相色谱-串联质谱法同时测定大鼠血浆中阿帕替尼与紫杉醇

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发布日期：2019-08-13 来源：分析测试学报浏览数：1543 人

作者

李天雪,胡玉涛,陈如洋,褚朝森

单位

1.江苏联合职业技术学院连云港中医药分院；2.连云港市药物研发共性技术中心

中文摘要:建立了同时定量测定大鼠血浆中阿帕替尼和紫杉醇的超高效液相色谱-串联质谱(UPLC-MS/MS)方法，并应用于药动学研究。血浆样品经固相萃取(SPE)处理。色谱柱为Agilent Zorbax Eclipse Plus C18柱(100 mm×2.1 mm，1.8 μm)，流动相为乙腈-0.1%甲酸溶液，体积流量0.4 mL/min，柱温40 ℃，进样量为3 μL。质谱采用电喷雾正离子源模式(ESI+)，多反应监测模式(MRM)进行定量测定。阿帕替尼和紫杉醇在0.5~1 500 μg/L范围内均呈良好的线性关系(r2≥0.998)，最低定量下限(LLOQ)均为0.5 μg/L，日内、日间精密度RSD≤8.4%，准确度为92.5%~107.1%，提取回收率为86.2%~95.1%，基质效应(86.6%~108.6%)不影响待测物血药浓度的测定。经方法学验证，该法快速灵敏，可同时对阿帕替尼和紫杉醇进行血药浓度监测，为临床联合用药研究提供了重要的分析手段。

中文关键词:阿帕替尼紫杉醇超高效液相色谱-串联质谱(UPLC-MS/MS) 定量分析药代动力学

Simultaneous Determination of Afatinib and Paclitaxel in Rat Plasma by UPLC-MS/MS

Abstract:An UPLC-MS/MS method was developed for the quantification of afatinib and paclitaxel in rat plasma.The method was also applied in the investigation on the pharmacokinetics of the analytes.The plasma samples were extracted by solid-phase extraction(SPE),and seperated on an Agilent Zorbax Eclipse Plus C18(100 mm×2.1 mm，1.8 μm) column with acetonitrile and water containing 0.1% formic acid as mobile phases at a flow rate of 0.4 mL/min,a column temperature of 40 ℃ and a sample injection of 3 μL.The quantification analysis was performed by MS with positive electrospray ionization(ESI+) source in multiple reaction monitoring(MRM) mode.The calibration curves for two analytes were linear over the concentration range of 0.5-1 500 μg/L,with correlation coefficients(r2) of 0.998 and the lower limits of quantitation(LLOQs) of 0.5 μg/L.The inter-day RSDs and intra-day RSDs were not more than 8.4%,and the accuracy ranged from 92.5% to 107.1%.The average recoveries were in the range of 86.2%-95.1%.The matrix effect values were sufficiently minimized to 86.6%-108.6%.The validated method is rapid and sensitive.It could be applied in the determination of afatinib and paclitaxel in plasma,and provide an analysis means for the clinical medication adjustment.

Key Words:afatinib paclitaxel UPLC-MS/MS quantification analysis pharmacokinetics

引用本文：李天雪,胡玉涛,陈如洋,褚朝森.超高效液相色谱-串联质谱法同时测定大鼠血浆中阿帕替尼与紫杉醇[J].分析测试学报,2018,37(4):477-481.

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